CN108815888B - Sedimentation tank for treating wastewater of white carbon black preparation process by sedimentation method - Google Patents
Sedimentation tank for treating wastewater of white carbon black preparation process by sedimentation method Download PDFInfo
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D21/02—Settling tanks with single outlets for the separated liquid
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- C01B33/00—Silicon; Compounds thereof
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Abstract
The invention relates to the technical field of white carbon black processes, in particular to a sedimentation tank for treating white carbon black process wastewater prepared by a sedimentation method, which comprises a primary sedimentation tank and a secondary sedimentation tank, wherein a feed inlet for putting quicklime is formed in the right end of the primary sedimentation tank, and a water inlet of a first pipeline is formed in the upper end of the feed inlet, so that the problems of upward and downward rolling of water in the primary sedimentation tank, poor sedimentation effect and long sedimentation period caused by the fact that the quicklime directly contacts with the wastewater to generate large amount of heat are avoided; still be equipped with buffer structure in the secondary sedimentation tank, buffer structure includes the plummer, and the baffler lower extreme is equipped with transfer passage, and transfer passage is located the middle level suspension layer department of secondary sedimentation tank, can not produce the impact in the secondary sedimentation tank to outside, and the supernatant that flows in is carried to the middle level suspension layer of secondary sedimentation tank via transfer passage and is guaranteed that the supernatant secondary clear liquid is not disturbed, guarantees the precipitation effect.
Description
The technical field is as follows:
the invention relates to the technical field of white carbon black processes, in particular to a sedimentation tank for treating wastewater of a white carbon black preparation process by a sedimentation method.
Background art:
white carbon black is an important reinforcing material in the rubber industry, and is called white carbon black because the microstructure and aggregate form of the white carbon black are similar to those of carbon black and the white carbon black has similar reinforcing performance in rubber. The first generation white carbon black is a traditional or "standard" white carbon black variety. The second generation is called high performance reinforcing white carbon black, which is Hengsil-988 high performance reinforcing white carbon black, and is a novel reinforcing material with high dispersibility and suitable for green tires. Energy conservation and environmental protection are two main subjects of the current society.
In the prior art, the precipitation method is adopted to prepare the white carbon black, the production cost is high, the direct discharge is mainly reflected in the treatment cost of wastewater, the environmental pollution is inevitably caused by direct discharge, and the method is not in line with the idea of modern industry, in the existing precipitation method for preparing the white carbon black, the process is complex, the energy consumption is high, the product rate is low, when the white carbon black is prepared by the precipitation method, concentrated sulfuric acid and sodium silicate react under the heating condition, and a finished product is obtained after the processes of precipitation, filtration, drying and the like to form certain wastewater, the wastewater is mainly produced in the filtration washing process, the main pollution factors of the wastewater are pH and SS, the annual output of the white carbon black of 5000 tons in the production process, and the wastewater generated in the filtration washing process reaches 53730m3A, the direct discharge of the waste water can cause harm to the environment, especially waste of water resources, simultaneously improves the water consumption, increases the water consumption cost, and filters out the mother liquor by using a filter pressIn the process, the direct discharge of the mother liquor causes environmental pollution.
The invention content is as follows:
the application aims to solve the problem that the yield of white carbon black prepared by a precipitation method is low and the pollution rate is high in the prior art;
another technical problem that will solve of this application provides a sedimentation tank for handling precipitation method preparation white carbon black technology waste water, solves among the prior art waste water treatment cost height, the big problem of the processing degree of difficulty. Realizes the cyclic utilization of the waste water and reduces the production cost.
The technical problem to be solved by the application is realized by adopting the following technical scheme: the preparation method of the white carbon black comprises the following steps:
s1: adding solid sodium silicate into a dissolving device, adding water, sealing the dissolving device, introducing steam until the steam pressure in the dissolving device reaches 120-150 cm of mercury, and after all the sodium silicate is dissolved, forming a solution with the specific gravity of 1.36-1.38 g/cm3Dilute sodium silicate solution, and putting the dilute sodium silicate solution into a reaction kettle;
s2: slowly conveying 98% concentrated sulfuric acid to a dilution tank through a pipeline for dilution to form a concentrated sulfuric acid solution with the specific gravity of 1.2-1.35 g/cm3The diluted sulfuric acid is prepared by mixing the diluted sulfuric acid prepared by the method with 10-11 m3The reaction solution is conveyed to a reaction kettle, mixed and stirred when the reaction temperature is controlled to be 30-32 ℃, kept stand for 1-3 hours for aging and generating seed crystals when the pH of the solution in the reaction kettle reaches 6.0-7.5, and then stirred to form a mixed solution;
s3: introducing high-temperature water vapor into the mixed solution obtained in the step S2 for heating, stopping introducing the high-temperature water vapor when the temperature of the solution in the reaction kettle is heated to 70-80 ℃, and adding the high-temperature water vapor with the specific gravity of 1.36-1.38 g/cm3When the pH of the solution in the reaction kettle is 11.0-11.5, stopping adding the dilute sodium silicate;
s4: and introducing high-temperature water vapor into the solution obtained after the reaction in the step S3 for heating, stopping introducing the high-temperature water vapor when the temperature of the solution in the reaction kettle is heated to 88-94 ℃, and introducing 98% sulfuric acid with the concentration of 0.52-0.7 m3Adding the solution at a flow rate of/h, and when the pH value of the solution in the reaction kettle is 3.0-5.0, finishing the synthesis and separating out precipitates in the reaction kettle;
s5: filtering, pulping and drying the precipitate to form primary white carbon black;
s6: fully dispersing the primary white carbon black prepared in the step S5 by using n-hexane, then adding a coupling reagent, and stirring and reacting for 6-48 hours at 20-80 ℃ under an anhydrous condition; after the reaction is finished, sequentially washing the reaction product by using n-hexane and ethanol, and drying the reaction product at the temperature of 30-200 ℃; the molar ratio of the primary white carbon black to the coupling reagent is 1 (0.01-0.1), wherein the coupling reagent is hexamethyldisilazane.
Preferably, the precipitate filtering step in the step S5 includes: filtering the suspension reacted in the step S4 by using a filter to remove mother liquor and recover sodium sulfate, then adding water to wash the filter cake until no precipitate is detected in the saturated barium hydroxide solution, and blowing the filter cake to discharge materials by using compressed air.
Preferably, the method also comprises the step of recycling the washed wastewater, which comprises the steps of conveying the wastewater generated by filtering in the step S5 into a sedimentation tank, adding quicklime for neutralization treatment, conveying the supernatant of the upper layer of the sedimentation tank into the step S5 for recycling after sedimentation, and periodically dehydrating and selling calcium sulfate formed by sedimentation in the sedimentation tank.
In this application, the sedimentation tank is including a sedimentation tank and secondary sedimentation tank, a sedimentation tank upper end is equipped with the first pipeline of carrying waste water, and a sedimentation tank right-hand member is equipped with the feed inlet that is used for puting in quick lime, the water inlet setting of first pipeline is in the upper end department of feed inlet, and one side that a sedimentation tank kept away from the feed inlet is equipped with the secondary sedimentation tank, secondary sedimentation tank and a sedimentation tank are carried to the secondary sedimentation tank via the second pipeline intercommunication, and the supernatant that forms in the primary sedimentation tank and after the sediment, the supernatant is the supernatant secondary clear liquid recycle who forms after the secondary sedimentation tank is depositd once more.
Preferably, the primary sedimentation tank bottom is equipped with the landslide, the higher end setting of landslide is in feed inlet department, and the bottom setting of landslide is kept away from the bottom of feed inlet one side at primary sedimentation tank than the bottom, one side that primary sedimentation tank is close to secondary sedimentation tank still is equipped with the accumulation pond that is used for collecting calcium sulfate, is equipped with on the primary sedimentation tank to be located the valve that is close to secondary sedimentation tank one side.
Preferably, the upper end of the landslide is also provided with a guide channel for guiding the wastewater and the quicklime to the middle part of the primary sedimentation tank.
Preferably, the first pipeline and the second pipeline are both provided with control switches.
Preferably, the middle part of the secondary sedimentation tank is horizontally provided with a drainage tube, the circumferential side wall of the drainage tube is provided with through holes, and one end of the drainage tube is communicated with one end of the second pipeline.
In this application, still be equipped with buffer gear in the secondary sedimentation tank, buffer gear sets up the one end that is close to the second pipeline at the secondary sedimentation tank, and buffer gear includes the plummer, the plummer allies oneself with the one end that is close to the second pipeline at the secondary sedimentation tank admittedly, and the plummer up end has been arranged along the secondary sedimentation tank lateral wall and has been assembled the platform, the one end that the second pipeline was kept away from to the plummer up end still is equipped with the baffler, the baffler lower extreme is equipped with transfer passage, transfer passage is located the middle level turbid layer department of secondary sedimentation tank.
Preferably, the convergence platform, the group partition plate and the bearing table are enclosed to form a buffer cavity.
Preferably, still be equipped with the tilter in the cushion chamber, the whole right-angle triangle toper form that is of tilter, the two right-angle sides of tilter inlay and establish in the platform that assembles and the plummer encloses the right angle department that closes the formation.
Preferably, the convergence platform and the bearing platform are rectangular integrally, and the length of the right-angle edge, which is perpendicular to the bearing platform and is attached to the convergence platform, on the inclined platform is 0.5-0.65 times of the height of the convergence platform.
Preferably, one end of the secondary sedimentation tank, which is far away from the second pipeline, is also provided with a discharge port, the discharge port is positioned in the middle of the upper secondary clear liquid of the secondary sedimentation tank, and the discharge port is provided with a control switch.
Preferably, the step S5 of recovering sodium sulfate from the mother liquor includes:
t1: evaporating and concentrating the mother liquor until the concentration of sodium sulfate reaches 25-30 Baume degrees;
t2: precisely filtering the sodium sulfate solution with the concentration of 25-30 Baume degrees obtained in the step T1 to obtain a refined sodium sulfate solution with the concentration of 25-30 Baume degrees;
t3: evaporating and crystallizing the refined sodium sulfate solution with the concentration of 25-30 Baume degrees to prepare anhydrous sodium sulfate;
t4: the anhydrous sodium sulfate generated by crystallization is separated out by an automatic discharge centrifuge, and the mother liquor returns to continue to be concentrated and crystallized.
Compared with the prior art, the beneficial effect of this application is:
1. according to the preparation method of the white carbon black, solid sodium silicate is added into a dissolving device, water is added, the dissolving device is sealed, steam is introduced to the steam pressure in the dissolving device, the introduced steam can accelerate the dissolution of the solid sodium silicate, and when the introduced pressure value is 120-150 cm, the heating of the solid sodium silicate can be accelerated, the molecular activity is improved, and the dissolving period is shortened;
2. in this application directly dilute concentrated sulfuric acid then carry to reation kettle in, for the convenience of the pH value in the control reation kettle, with dilute sulfuric acid conveying speed control at 10 ~ 11m3The pH value in the reaction kettle can be accurately controlled to be 6.0-7.5 through continuous mixing and stirring, and the problem that the pH value is not suitable to be controlled in the process of preparing the white carbon black by adopting a sulfuric acid precipitation method in the prior art is solved;
3. in the present application, in order to improve the yield of the traditional white carbon black, in step S4, 98% sulfuric acid is directly mixed by 0.52-0.7 m3The flow rate of the sulfuric acid is added into the solution, 98 percent concentrated sulfuric acid is added, so that a large amount of heat is released in the solution, the using amount of high-temperature water vapor is reduced, the sulfuric acid releases heat from the inside of the solution, the whole solution can be uniformly heated, the aging process is improved, the high yield is improved, and the problems of high using amount of the high-temperature water vapor and low yield caused by nonuniform heating of the solution due to adoption of dilute sulfuric acid in the prior art are solved; simultaneously adding primary white carbonThe white carbon black is subjected to modification treatment, so that the BET specific surface area of the white carbon black can be further enhanced;
4. in the application, the wastewater generated by filtering in the step S5 is conveyed into the sedimentation tank, and quicklime is added for neutralization treatment, so that acidic substances in the wastewater are neutralized, the pollution of the wastewater to the environment is reduced, and in the application, supernatant on the upper layer of the sedimentation tank is conveyed to the step S5 for cyclic utilization after sedimentation, so that the recovery rate of the wastewater is further improved, the use cost of water in the step S5 is reduced on the basis of reducing the discharge amount of the wastewater, the production cost is further reduced, meanwhile, calcium sulfate formed by sedimentation in the sedimentation tank is periodically dehydrated and sold, calcium sulfate in the wastewater is recovered, waste is changed into valuable, the modern industrial concept is met, and the cost of the white carbon black production process can be further reduced by selling the calcium sulfate;
5. in the application, step S5 is to recover sodium sulfate from the mother liquor, and the sodium sulfate solution is evaporated and concentrated by utilizing the waste heat of the boiler tail gas for producing high-temperature steam to produce anhydrous sodium sulfate, so that not only is the energy fully utilized, but also the anhydrous sodium sulfate is obtained;
6. the utility model provides a primary sedimentation tank, it is with the sour material of lime neutralization wastewater and generate calcium sulfate and precipitate, reach the purpose that reduces waste water pollution, primary sedimentation tank right-hand member is equipped with the feed inlet that is used for throwing in the lime, the water inlet of first pipeline sets up the upper end department at the feed inlet, the lime just fully contacts with waste water and mixes before not throwing into primary sedimentation tank, the steam that produces in its reaction process directly discharges at the feed inlet, the waste liquid after the full reaction enters into primary sedimentation tank, so, avoided the lime directly with waste water contact produce the big calorimetric problem that the water in the primary sedimentation tank rolls from top to bottom, the precipitation effect is poor, the problem of precipitation cycle length;
7. in the application, a landslide is arranged at the bottom of the primary sedimentation tank, the higher end of the landslide is arranged at the feed inlet, the lower end of the landslide is arranged at the bottom end of one side, far away from the feed inlet, of the primary sedimentation tank, the sediment generated by the reaction of wastewater and quicklime can slide to the bottom end of the left side of the primary sedimentation tank along the landslide and is matched with the accumulation tank, and the precipitated calcium sulfate can slide into the accumulation tank through a valve, so that the problem that the calcium sulfate is deposited at the bottom of the primary sedimentation tank and cannot be well treated is solved;
8. in the application, the primary sedimentation tank is used for further improving the sedimentation effect and avoiding the interference caused by the waste water thrown into the primary sedimentation tank, the upper end of the landslide is also provided with a guide channel for guiding the waste water and the quick lime to the middle part of the primary sedimentation tank, when the heat generated by the reaction of the waste water and the quick lime enters the primary sedimentation tank, the heat is limited in the guide channel, the impact of the waste water, the quick lime and corresponding reactants on the waste water in the primary sedimentation tank is limited in the guide channel, the waste water precipitation at other places except the guide channel cannot be interfered, the output end of the guide channel is positioned in the middle position of the primary sedimentation tank, namely the upper layer of the suspension layer is supernatant, the waste water, the quick lime and the reactants are conveyed to the place to be sedimentated, the supernatant is ensured not to be interfered, and the sedimentation effect is ensured;
9. in the application, in order to reduce wastewater pollution, the supernatant is conveyed to a secondary sedimentation tank for secondary sedimentation, the wastewater in the secondary sedimentation tank is also divided into three layers, the three layers comprise the supernatant, a middle suspension layer and a lower sedimentation layer, the circumferential side wall of a drainage tube in the middle of the secondary sedimentation tank is provided with a through hole, the middle position is arranged at the suspension layer, and the through hole which can be arranged can slowly convey the supernatant into the secondary sedimentation tank for sedimentation, so that the suspension layer and the supernatant can not be mixed, and the sedimentation effect is reduced;
10. in the application, in order to reduce the impact and influence of the supernatant conveyed from the primary sedimentation tank on the secondary sedimentation tank, a buffer structure is further arranged in the secondary sedimentation tank, the buffer structure comprises a bearing platform, a conveying channel is arranged at the lower end of the baffle plate, the conveying channel is positioned at the middle-layer suspension layer of the secondary sedimentation tank, water conveyed from the primary sedimentation tank is limited in a cavity formed by the combination of the combination baffle plate and the secondary sedimentation tank, the impact on the external secondary sedimentation tank cannot be generated, the inflowing supernatant is conveyed to the middle-layer suspension layer of the secondary sedimentation tank through the conveying channel, the upper-layer secondary supernatant is ensured not to be interfered, and the sedimentation effect is ensured;
11. in the application, the convergence platform, the group partition plates and the bearing platform are enclosed to form a buffer cavity, and the buffer cavity and the convergence platform are combined to form a step-shaped structure, so that the problem that supernatant falls on the convergence platform and flows into a conveying channel to enter a suspension layer of a secondary sedimentation tank is solved, and sediment in the supernatant flowing into the convergence platform slowly flows into the buffer cavity along the surface of the convergence platform and is deposited at the bottom of the secondary sedimentation tank;
12. in the application, in order to play a role of buffering, so that the supernatant liquid slowly flows into a suspension layer of a secondary sedimentation tank, a tilting table is further arranged in a buffer cavity, the tilting table is integrally in a right-angled triangular cone shape, two right-angled edges of the tilting table are embedded at a right-angled position formed by the convergence platform and the bearing platform in an enclosing manner, the tilting table is arranged, the impact when the supernatant liquid enters the buffer cavity is reduced, the impact can cause the precipitate in the supernatant liquid to be scattered and distributed, the sedimentation time is prolonged, the sedimentation effect is reduced, the supernatant liquid can have a force of entering the suspension layer of the secondary sedimentation tank, the blockage caused by the accumulation of the precipitate in the supernatant liquid in the buffer cavity is avoided, namely, the tilting table is arranged, the precipitate in the supernatant liquid can move along the surface of the tilting table, when the supernatant liquid enters the suspension layer, the precipitate in the supernatant liquid can be directly precipitated and enter the precipitation layer, the precipitation effect is improved.
Description of the drawings:
FIG. 1 is a schematic view of the structure of a sedimentation tank according to the present invention;
FIG. 2 is a schematic structural view of a secondary sedimentation tank;
FIG. 3 is a schematic view of a buffer mechanism;
FIG. 4 is a schematic view of a buffer mechanism;
in the figure: 10-primary sedimentation tank; 11-a first pipeline; 12-feeding port; 13-supernatant liquor; 14-landslide; 15-an accumulation pool; 16-valves; 17-a guide channel; 18-drainage tube; 20-secondary sedimentation tank; 21-a second pipeline; 22-upper-layer secondary clear liquid; 23-a discharge port; 30-a buffer mechanism; 31-a bearing platform; 32-a convergence platform; 33-group of partition boards; 34-a conveying channel; 35-buffer cavity; 36-inclined table.
The specific implementation mode is as follows:
in order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the invention is further clarified with the specific embodiments.
Example 1:
the preparation method of the white carbon black comprises the following steps:
s1: adding solid sodium silicate into a dissolving device, adding water, sealing the dissolving device, introducing steam until the steam pressure in the dissolving device reaches 120cm Hg, and dissolving the sodium silicate to obtain the sodium silicate with a specific gravity of 1.37g/cm3Dilute sodium silicate solution, and putting the dilute sodium silicate solution into a reaction kettle;
s2: slowly delivering 98% concentrated sulfuric acid to a dilution tank through a pipeline for dilution to form a product with the specific gravity of 1.27g/cm3Diluted sulfuric acid of (2), the diluted sulfuric acid formed in the above preparation is added at a concentration of 10.5m3The solution is conveyed into a reaction kettle for one hour, mixed and stirred when the reaction temperature is controlled to be 31 ℃, kept stand for 2 hours for aging and generating seed crystals when the pH value of the solution in the reaction kettle reaches 7, and then stirred to form a mixed solution;
s3: introducing high-temperature water vapor into the mixed solution obtained in the step S2 for heating, stopping introducing the high-temperature water vapor when the temperature of the solution in the reaction kettle is heated to 75 ℃, and adding the water vapor with the specific gravity of 1.37g/cm3When the pH of the solution in the reaction kettle is 11.25, stopping adding the dilute sodium silicate;
s4: then introducing high-temperature water vapor into the solution reacted in the step S3 for heating, stopping introducing the high-temperature water vapor when the temperature of the solution in the reaction kettle is heated to 91 ℃, and introducing 98% sulfuric acid with the concentration of 0.61m3Adding the solution at a flow rate of/h, and when the pH value of the solution in the reaction kettle is 4.0, finishing the synthesis and separating out precipitates in the reaction kettle;
s5: filtering, pulping and drying the precipitate to form primary white carbon black;
s6: fully dispersing the primary white carbon black prepared in the step S5 by using n-hexane, then adding a coupling reagent, and stirring and reacting for 6-48 hours at 20-80 ℃ under an anhydrous condition; after the reaction is finished, sequentially washing the reaction product by using n-hexane and ethanol, and drying the reaction product at the temperature of 30-200 ℃; the molar ratio of the primary white carbon black to the coupling reagent is 1 (0.01-0.1), wherein the coupling reagent is hexamethyldisilazane.
Example 2:
the content of this embodiment is basically the same as that of embodiment 1, and the same parts are not described again, except that: step S1, adding solid sodium silicate into a dissolving device, adding water, sealing the dissolving device, introducing steam until the steam pressure in the dissolving device reaches 125cm Hg, and dissolving all the sodium silicate to obtain the sodium silicate with the specific gravity of 1.37g/cm3And (3) diluting the sodium silicate solution, and putting the diluted sodium silicate solution into a reaction kettle.
Example 3:
the content of this embodiment is basically the same as that of embodiment 1, and the same parts are not described again, except that: step S1, adding solid sodium silicate into a dissolving device, adding water, sealing the dissolving device, introducing steam until the steam pressure in the dissolving device reaches 150cm Hg, and dissolving all the sodium silicate to obtain the sodium silicate with the specific gravity of 1.37g/cm3And (3) diluting the sodium silicate solution, and putting the diluted sodium silicate solution into a reaction kettle.
Example 4:
the content of this embodiment is basically the same as that of embodiment 1, and the same parts are not described again, except that: step S1, adding solid sodium silicate into a dissolving device, adding water, sealing the dissolving device, introducing steam until the steam pressure in the dissolving device reaches 160cm Hg, and dissolving all the sodium silicate to obtain the sodium silicate with the specific gravity of 1.37g/cm3And (3) diluting the sodium silicate solution, and putting the diluted sodium silicate solution into a reaction kettle.
Example 5:
the content of this embodiment is basically the same as that of embodiment 1, and the same parts are not described again, except that: in step S1, solid sodium silicate is added into a dissolving device, water is added into the dissolving device, the dissolving device is sealed, and steam is introduced until the steam pressure in the dissolving device reaches 110cm Hg.
The white carbon black prepared in examples 1 to 5 was tested, and the test results are shown in table 1:
TABLE 1
Example 6:
the content of the present embodiment is substantially the same as that of embodiment 2, and the same points are not repeated, except that: step S4: then introducing high-temperature water vapor into the solution reacted in the step S3 for heating, stopping introducing the high-temperature water vapor when the temperature of the solution in the reaction kettle is heated to 91 ℃, and introducing 98% sulfuric acid with the volume of 0.52m3The flow rate of the solution is added into the solution, when the pH value of the solution in the reaction kettle is 4.0, the synthesis is finished, and precipitates are separated out in the reaction kettle.
Example 7:
the content of the present embodiment is substantially the same as that of embodiment 2, and the same points are not repeated, except that: step S4: then introducing high-temperature water vapor into the solution reacted in the step S3 for heating, stopping introducing the high-temperature water vapor when the temperature of the solution in the reaction kettle is heated to 91 ℃, and introducing 98% sulfuric acid with the concentration of 0.61m3The flow rate of the solution is added into the solution, when the pH value of the solution in the reaction kettle is 4.0, the synthesis is finished, and precipitates are separated out in the reaction kettle.
Example 8:
the content of the present embodiment is substantially the same as that of embodiment 2, and the same points are not repeated, except that: step S4: then introducing high-temperature water vapor into the solution reacted in the step S3 for heating, stopping introducing the high-temperature water vapor when the temperature of the solution in the reaction kettle is heated to 91 ℃, and introducing 98% sulfuric acid with the volume of 0.7m3The flow rate of the solution is added into the solution, when the pH value of the solution in the reaction kettle is 4.0, the synthesis is finished, and precipitates are separated out in the reaction kettle.
Example 9:
the content of the present embodiment is substantially the same as that of embodiment 2, and the same points are not repeated, except that: step S4: then introducing high-temperature water vapor into the solution reacted in the step S3 for heating, stopping introducing the high-temperature water vapor when the temperature of the solution in the reaction kettle is heated to 91 ℃, and introducing 98% sulfuric acid with the concentration of 0.4m3The flow rate of the solution is added into the solution, when the pH value of the solution in the reaction kettle is 4.0, the synthesis is finished, and precipitates are separated out in the reaction kettle.
Example 10:
the content of the present embodiment is substantially the same as that of embodiment 2, and the same points are not repeated, except that: step S4: then introducing high-temperature water vapor into the solution reacted in the step S3 for heating, stopping introducing the high-temperature water vapor when the temperature of the solution in the reaction kettle is heated to 91 ℃, and introducing 98% sulfuric acid with the concentration of 0.8m3The flow rate of the solution is added into the solution, when the pH value of the solution in the reaction kettle is 4.0, the synthesis is finished, and precipitates are separated out in the reaction kettle.
Comparative example 1:
this comparative example is the white carbon black prepared under application No. CN 201210476263.0.
The white carbon black prepared in the examples 6 to 10 is subjected to performance test, and the test results are shown in table 2:
TABLE 2
Example 11:
the content of the present embodiment is substantially the same as that of embodiment 6, and the same points are not repeated, except that: as shown in fig. 1, the system further comprises a primary sedimentation tank 10, a first pipeline 11 for conveying wastewater is arranged at the upper end of the primary sedimentation tank 10, a feed inlet 12 for putting quicklime is arranged at the right end of the primary sedimentation tank 10, a water inlet of the first pipeline 11 is arranged at the upper end of the feed inlet 12, a secondary sedimentation tank 20 is arranged at one side of the primary sedimentation tank 10, which is far away from the feed inlet 12, the secondary sedimentation tank 20 is communicated with the primary sedimentation tank 10 through a second pipeline 21, a supernatant 13 formed in the primary sedimentation tank 10 after neutralization and sedimentation is conveyed to the secondary sedimentation tank 20, and a supernatant 22 formed after the supernatant 13 is settled in the secondary sedimentation tank 20 again is recycled, so that the primary sedimentation tank 10 provided by the application uses acidic substances in the quicklime and in the wastewater to generate calcium sulfate sediment so as to achieve the purpose of reducing wastewater pollution, the feed inlet 12 for putting the quicklime is arranged at the right end of the primary sedimentation, the water inlet setting of first pipeline 11 is in the upper end department of feed inlet 12, and quick lime just fully contacts with waste water before not throwing into once sedimentation tank 10 and mixes, and the steam that produces in its reaction directly discharges in feed inlet 12 department, and waste liquid after the full reaction enters into once sedimentation tank 10 in, so, has evaded quick lime and has directly produced the big heat with waste water contact and lead to rolling about the water in the sedimentation tank 10 once, and the precipitation effect is poor, the problem of precipitation cycle length.
Example 12:
as shown in fig. 1, the content of this embodiment is substantially the same as that of embodiment 11, and the same points are not repeated, except that: the bottom of the primary sedimentation tank 10 is provided with a landslide 14, the higher end of the landslide 14 is arranged at the feed inlet 12, the lower end of the landslide 14 is arranged at the bottom end of the primary sedimentation tank 10 far away from the feed inlet 12, one side of the primary sedimentation tank 10 close to the secondary sedimentation tank 20 is also provided with an accumulation tank 15 for collecting calcium sulfate, the primary sedimentation tank 10 is provided with a valve 16 close to one side of the secondary sedimentation tank 20, thus, in the application, the bottom of the primary sedimentation tank 10 is provided with the landslide 14, the higher end of the landslide 14 is arranged at the feed inlet 12, the lower end of the landslide 14 is arranged at the bottom end of the primary sedimentation tank 10 far away from the feed inlet 12, the sediment generated by the reaction of the waste water and the quicklime can slide to the bottom end of the left side of the primary sedimentation tank 10 along the landslide 14 and is matched with the accumulation tank 15, the precipitated calcium sulfate can slide into the accumulation, the problem of poor treatment.
Example 13:
as shown in fig. 1, the content of the present embodiment is substantially the same as that of embodiment 12, and the same points are not repeated, except that: the upper end of the landslide 14 is further provided with a guide channel 17 for guiding the wastewater and the quicklime to the middle of the primary sedimentation tank 10, and the first pipeline 11 and the second pipeline 21 are both provided with control switches, so in the application, the primary sedimentation tank 10 is used for further improving the sedimentation effect and avoiding the interference caused by the wastewater fed into the primary sedimentation tank 10, the upper end of the landslide 14 is further provided with a guide channel 17 for guiding the wastewater and the quicklime to the middle of the primary sedimentation tank 10, when the heat generated by the reaction of the wastewater and the quicklime enters the primary sedimentation tank 10, the heat is limited in the guide channel 17, the impact of the wastewater, the quicklime and corresponding reactants on the wastewater in the primary sedimentation tank 10 is limited in the guide channel 17, the precipitation of the wastewater at other places except the guide channel 17 cannot be interfered, and the output end of the guide channel 17 is positioned in the middle of the primary sedimentation tank 10, namely in the suspension layer of the primary sedimentation tank 110, the supernatant liquid 13 is arranged on the upper layer of the suspension layer, and wastewater, quicklime and reactants which are conveyed to the upper layer are precipitated, so that the supernatant liquid 13 is ensured not to be interfered, and the precipitation effect is ensured.
Example 14:
as shown in fig. 1, the content of this embodiment is substantially the same as that of embodiment 13, and the same points are not repeated, except that: in the application, in order to reduce the wastewater pollution, the supernatant 13 is conveyed to the secondary sedimentation tank 20 for secondary sedimentation, the wastewater in the secondary sedimentation tank 20 is also divided into three layers, including an upper secondary clear liquid 22, a middle suspension layer and a lower sedimentation layer, the circumferential side wall of the drainage tube 18 in the middle of the secondary sedimentation tank 20 is provided with a through hole, the middle position is arranged at the suspension layer, the through hole which can be arranged can slowly convey the supernatant 13 into the secondary sedimentation tank 20 for sedimentation, so that the suspension layer and the upper secondary clear liquid 22 can not be mixed, the sedimentation effect is reduced, specifically, the secondary sedimentation tank 20 is arranged on one side of the primary sedimentation tank 10 far away from the feed port 12, the secondary sedimentation tank 20 and the primary sedimentation tank 10 are communicated through a second pipeline 21, the supernatant 13 formed in the primary sedimentation tank 10 after sedimentation is conveyed to the secondary sedimentation tank 20, the supernatant 22 formed after the secondary sedimentation tank 20 is subjected to secondary sedimentation, a drainage tube 18 is horizontally arranged in the middle of the secondary sedimentation tank 20, through holes are formed in the circumferential side wall of the drainage tube 18, and one end of the drainage tube 18 is communicated with one end of a second pipeline 21.
Example 15:
as shown in fig. 2, the content of the present embodiment is substantially the same as that of embodiment 12, and the same points are not repeated, except that: the secondary sedimentation tank 20 is also internally provided with a buffer mechanism 30, the buffer mechanism 30 is arranged at one end of the secondary sedimentation tank 20 close to the second pipeline 21, the buffer mechanism 30 comprises a bearing platform 31, the bearing platform 31 is fixedly connected at one end of the secondary sedimentation tank 20 close to the second pipeline 21, the upper end surface of the bearing platform 31 is provided with a convergence platform 32 along the side wall of the secondary sedimentation tank 20, one end of the upper end surface of the bearing platform 31 far away from the second pipeline 21 is also provided with a baffle plate 33, the lower end of the baffle plate 33 is provided with a conveying channel 34, the conveying channel 34 is positioned at the suspension layer of the secondary sedimentation tank 20, thus, in the application, in order to reduce the impact and influence of the upper layer clear liquid 13 conveyed from the primary sedimentation tank 10 on the secondary sedimentation tank 20, the buffer mechanism 30 is also arranged in the secondary sedimentation tank 20, the buffer mechanism 30 comprises the bearing platform 31, the lower end of the baffle plate 33 is provided with the conveying channel 34, the conveying channel, the water delivered from the primary sedimentation tank 10 is limited in a cavity formed by the group partition plate 33 and the secondary sedimentation tank 20, the impact on the outside secondary sedimentation tank 20 is avoided, the inflowing supernatant liquid 13 is delivered to the middle layer suspension layer of the secondary sedimentation tank 20 through the delivery channel 34, the upper layer secondary clear liquid 22 is ensured not to be interfered, and the sedimentation effect is ensured.
Example 16:
as shown in fig. 3, the content of this embodiment is substantially the same as that of embodiment 15, and the same points are not repeated, except that: still enclose to close including converging platform 32, group's baffle 33 and plummer 31 and be formed with cushion chamber 35, so, in this application, it closes to close to be formed with cushion chamber 35 to converge platform 32, group's baffle 33 and plummer 31, this cushion chamber 35 and converge platform 32 and combine to form step-like structure to reduce supernatant 13 and fall to converge the platform 32 and flow into transfer passage 34 and get into the big problem of suspension layer impact of secondary sedimentation tank 20, the deposit that flows into in the supernatant 13 that converges platform 32 can flow into cushion chamber 35 and deposit in secondary sedimentation tank 20 bottom slowly along converging platform 32 surface.
Example 17:
as shown in fig. 4, the content of this embodiment is substantially the same as that of embodiment 16, and the same points are not repeated, except that: the buffer cavity 35 is also internally provided with an inclined platform 36, the inclined platform 36 is integrally in a right-angled triangular conical shape, two right-angled edges of the inclined platform 36 are embedded at a right-angled position formed by enclosing the convergence platform 32 and the bearing platform 31, the convergence platform 32 and the bearing platform 31 are integrally in a rectangular shape, the length of the right-angled edge which is perpendicular to the bearing platform 31 and is attached to the convergence platform 32 on the inclined platform 36 is 0.6 times the length of the height of the convergence platform 32, one end of the secondary sedimentation tank 20 far away from the second pipeline 21 is also provided with a discharge port 23, the discharge port 23 is positioned at the middle position of the upper secondary clear liquid 22 of the secondary sedimentation tank 20, and the discharge port 23 is provided with a control switch, so that in the application, in order to play a role of buffering, the upper clear liquid slowly flows into a suspension layer of the secondary sedimentation tank 20, the inclined platform 36 is also arranged in the buffer cavity 35, the inclined platform 36 is integrally in a right-angled triangular conical shape, two right-angled edges of the, the inclined platform 36 that is equipped with has not only reduced the impact when supernatant 13 gets into cushion chamber 35, this impact can lead to the precipitate in the supernatant 13 to scatter in disorder and distribute, the extension settling time, reduce the precipitation effect, and can also make supernatant 13 possess the power that gets into secondary sedimentation tank 20 suspension layer, avoid the precipitate in the supernatant 13 to gather and cause the jam in cushion chamber 35, that is to say, the inclined platform 36 that is equipped with can make the precipitate in the supernatant 13 along inclined platform 35 surface motion, when supernatant 13 gets into the suspension layer, the precipitate in the supernatant 13 can directly precipitate and get into the precipitate layer, improve the precipitation effect.
Example 18:
the content of the present embodiment is substantially the same as that of embodiment 17, and the same points are not repeated, except that: the step S5 of recovering sodium sulfate from the mother liquor includes:
t1: evaporating and concentrating the mother liquor until the concentration of sodium sulfate reaches 27 Baume degrees;
t2: finely filtering the sodium sulfate solution with the concentration of 27 Baume degrees obtained in the step T1 to obtain a refined sodium sulfate solution with the concentration of 27 Baume degrees;
t3: evaporating and crystallizing the refined sodium sulfate solution with the concentration of 27 Baume degrees to prepare anhydrous sodium sulfate;
t4: the anhydrous sodium sulfate generated by crystallization is separated out by an automatic discharge centrifuge, and the mother liquor returns to continue to be concentrated and crystallized.
The foregoing shows and describes the general principles, essential features, and inventive features of this invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A sedimentation tank for treating white carbon black preparation process wastewater by a sedimentation method is characterized by comprising a primary sedimentation tank and a secondary sedimentation tank, wherein a first pipeline for conveying wastewater is arranged at the upper end of the primary sedimentation tank, a feed inlet for putting quicklime is arranged at the right end of the primary sedimentation tank, a water inlet of the first pipeline is arranged at the upper end of the feed inlet, a secondary sedimentation tank is arranged on one side of the primary sedimentation tank, which is far away from the feed inlet, the secondary sedimentation tank and the primary sedimentation tank are communicated through a second pipeline, supernatant liquor formed in the primary sedimentation tank after the primary sedimentation tank and the sedimentation is conveyed to the secondary sedimentation tank, and the supernatant liquor formed after the supernatant liquor is sedimentated again in the secondary sedimentation tank is recycled;
the bottom of the primary sedimentation tank is provided with a landslide, the higher end of the landslide is arranged at the feed inlet, the lower end of the landslide is arranged at the bottom end of one side of the primary sedimentation tank far away from the feed inlet, one side of the primary sedimentation tank close to the secondary sedimentation tank is also provided with an accumulation tank for collecting calcium sulfate, and the primary sedimentation tank is provided with a valve positioned at one side close to the secondary sedimentation tank;
still be equipped with buffer gear in the secondary sedimentation tank, buffer gear sets up the one end that is close to the second pipeline at the secondary sedimentation tank, and buffer gear includes the plummer, the plummer links firmly the one end that is close to the second pipeline at the secondary sedimentation tank, and the plummer up end has been arranged along the secondary sedimentation tank lateral wall and has been assembled the platform, the one end that the second pipeline was kept away from to the plummer up end still is equipped with the baffler, the baffler lower extreme is equipped with transfer passage, transfer passage is located the middle level turbid layer department of secondary sedimentation tank.
2. The sedimentation tank for treating white carbon black preparation process wastewater by a sedimentation method according to claim 1, wherein a guide channel for guiding the wastewater and quicklime together to the middle part of the primary sedimentation tank is further arranged at the upper end of the landslide.
3. The sedimentation tank for treating white carbon black preparation process wastewater by using a sedimentation method according to claim 1, wherein control switches are arranged on the first pipeline and the second pipeline.
4. The sedimentation tank for treating white carbon black preparation process wastewater by using a sedimentation method according to claim 1, wherein a drainage tube is further horizontally arranged in the middle of the secondary sedimentation tank, through holes are formed in the circumferential side wall of the drainage tube, and one end of the drainage tube is communicated with one end of a second pipeline.
5. The sedimentation tank for treating white carbon black preparation process wastewater by a sedimentation method according to claim 1, wherein the convergence platform, the group partition plate and the bearing table enclose to form a buffer cavity.
6. The sedimentation tank for treating white carbon black preparation process wastewater by using a sedimentation method according to claim 5, wherein an inclined table is further arranged in the buffer chamber, the inclined table is integrally in a right-angle triangular cone shape, and two right-angle sides of the inclined table are embedded at a right angle formed by the enclosing of the convergence platform and the bearing platform.
7. The sedimentation tank for treating white carbon black preparation process wastewater by using a sedimentation method according to claim 6, wherein the convergence platform and the bearing table are rectangular as a whole, and the length of the right-angle side, which is perpendicular to the bearing table and is attached to the convergence platform, on the inclined table is 0.5-0.65 times the height of the convergence platform.
8. The sedimentation tank for treating white carbon black preparation process wastewater by using a sedimentation method according to claim 1, wherein a discharge port is further formed in one end of the secondary sedimentation tank, which is far away from the second pipeline, the discharge port is located in the middle of the upper secondary clear liquid of the secondary sedimentation tank, and a control switch is arranged on the discharge port.
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| CN101020588A (en) * | 2006-02-13 | 2007-08-22 | 杨合理 | Calcium carbonate coagulating technology for treating waste water |
| CN101618292A (en) * | 2008-11-10 | 2010-01-06 | 李元胜 | System for comprehensive utilization of three industrial wastes |
| US9962631B2 (en) * | 2009-01-23 | 2018-05-08 | Stuart J Ward | Effluent weir system |
| CN201832456U (en) * | 2010-10-30 | 2011-05-18 | 山西太钢不锈钢股份有限公司 | Water treatment sedimentation apparatus |
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